DE3923983A1 - METHOD AND DEVICE FOR DETERMINING ELEMENTS - Google Patents

METHOD AND DEVICE FOR DETERMINING ELEMENTS

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Publication number
DE3923983A1
DE3923983A1 DE19893923983 DE3923983A DE3923983A1 DE 3923983 A1 DE3923983 A1 DE 3923983A1 DE 19893923983 DE19893923983 DE 19893923983 DE 3923983 A DE3923983 A DE 3923983A DE 3923983 A1 DE3923983 A1 DE 3923983A1
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Prior art keywords
filter
induction furnace
atomic absorption
ceramic
elements
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DE19893923983
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German (de)
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DE3923983C2 (en
Inventor
Hermann R Trabert
Cvetko Krajina
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Priority to DE19893923983 priority Critical patent/DE3923983C2/en
Priority to EP19900911638 priority patent/EP0436008A1/en
Priority to JP51083190A priority patent/JPH04503412A/en
Priority to PCT/EP1990/001146 priority patent/WO1991001487A1/en
Publication of DE3923983A1 publication Critical patent/DE3923983A1/en
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Publication of DE3923983C2 publication Critical patent/DE3923983C2/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/74—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flameless atomising, e.g. graphite furnaces
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/74—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flameless atomising, e.g. graphite furnaces
    • G01N2021/745—Control of temperature, heating, ashing

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

This invention relates to a process and a device for the determination of elements by means of atomic absorption and X-ray fluorescent analysis. The process according to this invention comprises the three steps evaporization of the sample with concurrent oxidation, collection of the oxides in a filter and measurement of the element concentrations by ashing the filter in an atomic absorption spectrophotometer or analysis of the filter in an X-ray spectrometer or an optical emission spectrophotometer. The induction furnace has been especially adapted.

Description

Die Erfindung betrifft ein Verfahren und eine Vorrichtung zur Bestimmung von Elementen mittels dem Atomabsorptionsverfahren, ICP oder anderen analytischen Methoden.The invention relates to a method and an apparatus for determination of elements using the atomic absorption process, ICP or others analytical methods.

Bekannte Atomabsorptionsverfahren bestimmen die Elemente in kompliziert zusammengesetzten Materialien mittels Atomisierung der Proben in einer Flamme oder in elektrothermischen Atomisierern. Diese Methoden haben deutliche Nachteile. Ohne die vorherige Konzentration der direkt analysierten Elemente ist die Nachweisgrenze zu niedrig. Geringe Präzision der Meßergebnisse ergibt sich durch Matrix- und Inter­ ferenzeffekte anderer Elemente. Um die Nachweisgrenze zu erhöhen und die Genauigkeit der Messungen zu verbessern, wird ein neues erfindungsgemäßes Konzentrationsverfahren im Zusammenhang mit der Atomabsorptionsmethode, ICP und anderen analytischen Methoden (z.B. Röntgenanalysator) verwandt.Known atomic absorption processes determine the elements in a complicated manner composite materials by atomizing the samples in one Flame or in electrothermal atomizers. Have these methods clear disadvantages. Without the previous concentration of the direct analyzed elements the detection limit is too low. Low Precision of the measurement results is given by matrix and inter ference effects of other elements. To increase the detection limit and the To improve the accuracy of the measurements is a new invention Concentration process in connection with the atomic absorption method, ICP and other analytical methods (e.g. X-ray analyzer) are used.

Das Atomabsorptionsverfahren ohne die chemische Probenvorbereitung ist aus der DE-32 23 334 bekannt. Bei diesem Verfahren werden die Proben gepreßt und in einem Graphitbehälter mit geschlossenen Öffnungen plaziert. Der Behälter wird in die Flamme eines Plasmabrenners gebracht, wobei die Probe bei hohen Temperaturen verbrannt wird. Bei diesem Ver­ fahrensschritt tritt eine teilweise fraktionierte Evaporisation der Elemente in der Gasphase auf.The atomic absorption process without chemical sample preparation is known from DE-32 23 334. In this procedure, the samples pressed and in a graphite container with closed openings placed. The container is placed in the flame of a plasma torch, the sample being burned at high temperatures. With this ver a partial fractional evaporation of the Elements in the gas phase.

Aufgabe des erfindungsgemäßen Verfahrens und der erfindungsgemäßen Vorrichtung ist es, die oben genannten Nachteile zu überwinden. Object of the inventive method and the inventive The device is to overcome the disadvantages mentioned above.  

Das erfindungsgemäße Verfahren ist auf Elemente oder deren Oxide, welche eine höhere Volatilität bei höheren Temperaturen als die Matrix besitzt, anwendbar.The method according to the invention is based on elements or their oxides has higher volatility at higher temperatures than the matrix, applicable.

Dies betrifft folgende Elemente: Al, Ag, As, B, Ba, Bi, Ca, Cd, Ce, Ga, Ge, Hg, In, K, Li, Mg, Mn, Na, Nb, Os, P, Pb, Rb, Re, Ru, Se, Si, Sn, Sr, Ta, Te, Zn.This affects the following elements: Al, Ag, As, B, Ba, Bi, Ca, Cd, Ce, Ga, Ge, Hg, In, K, Li, Mg, Mn, Na, Nb, Os, P, Pb, Rb, Re, Ru, Se, Si, Sn, Sr, Ta, Te, Zn.

Der für das erfindungsgemäße Verfahren benötigte Induktionsofen, welcher aus dem Stand der Technik bekannt ist, wurde diesem Verfahren speziell angepaßt. Näheres kann der Figurenbeschreibung und den Ansprüchen ent­ nommen werden.The induction furnace required for the method according to the invention, which is known from the prior art, this method was special customized. More details can be found in the description of the figures and the claims be taken.

Das erfindungsgemäße Verfahren weist die drei VerfahrensschritteThe method according to the invention has the three method steps

  • - Verflüchtigung der Proben bei gleichzeitiger Oxidation,Volatilization of the samples with simultaneous oxidation,
  • - Auffangen der Oxide in einem Filter und- Collecting the oxides in a filter and
  • - Messung der Elementkonzentrationen durch Veraschung des Filters in einem Atomabsorptionsspektrophotometer oder der direkten Messung durch einen Röntgenspektrometer auf. Die Verfahrensschritte werden im einzelnen ebenfalls in den Ansprüchen und in der Figurenbeschreibung näher erläutert.- Measurement of element concentrations by ashing the filter in an atomic absorption spectrophotometer or direct measurement by an x-ray spectrometer. The process steps are in individual also in the claims and in the description of the figures explained in more detail.

Weitere erfindungsgemäße Vorteile ergeben sich aus der Figurenbe­ schreibung, welche nur im beschreibenden und nicht im begrenzenden Sinn aufgefaßt werden soll.Further advantages according to the invention result from the figure writing, which is only in the descriptive and not in the limiting sense should be understood.

Es zeigen:Show it:

Fig. 1 einen Schnitt durch den erfindungsgemäßen Induktionsofen; und FIG. 1 is a section through the induction furnace according to the invention; and

Fig. 2 ein Flußdiagramm der Verfahrensschritte. Fig. 2 is a flow diagram of the process steps.

Fig. 1 zeigt einen Schnitt durch einen Induktionsofen, welcher in seinen Grundelementen an sich bekannt ist. Der Keramiktiegel 16 zur Aufnahme der zu untersuchenden Probe sitzt auf einem Sockel 18 innerhalb der Quarz­ röhre 12. Um den Keramiktiegel 16 herum befindet sich eine Erwärmungs­ vorrichtung 14, welche induktiv oder auf andere Weise wirken kann. Die Quarzröhre 12 wird nach oben durch den Metallzylinder 24 sowie nach unten durch die Bodenabdeckung 20 abgeschlossen, wobei die Dichtungen 34 zwischen der Quarzröhre 12 und dem Metallzylinder 24 bzw. der Boden­ abdeckung 20 einen dichten Abschluß gewährleisten. Über die Röhre 22, welche in der Bodenabdeckung 20 angeordnet ist, wird ein Trägergas in dem Innenraum des Induktionsofens 10 geleitet. Über die erfindungsgemäße Röhre 26, welche durch eine Öffnung im Metallzylinder 24 in den Innenraum des Induktionsofens 10 oberhalb des Keramiktiegels ragt, wird als Reaktionsgas Sauerstoff (O2) eingeleitet. Fig. 1 shows a section through an induction furnace, which is known per se in its basic elements. The ceramic crucible 16 for receiving the sample to be examined sits on a base 18 within the quartz tube 12th Around the ceramic crucible 16 there is a heating device 14 , which can act inductively or in another way. The quartz tube 12 is closed at the top by the metal cylinder 24 and at the bottom by the base cover 20 , the seals 34 between the quartz tube 12 and the metal cylinder 24 or the base cover 20 ensuring a tight seal. A carrier gas is passed in the interior of the induction furnace 10 via the tube 22 , which is arranged in the base cover 20 . Oxygen (O 2 ) is introduced as the reaction gas via the tube 26 according to the invention, which projects through an opening in the metal cylinder 24 into the interior of the induction furnace 10 above the ceramic crucible.

Im oberen Abschnitt des Metallzylinders 24 ist ein erfindungsgemäßer Filter 30 angebracht, welcher mittels der Wechselvorrichtung 36 entnommen und erneuert werden kann. Der Filter 30 dient zum Auffangen der bei dem Verbrennungsvorgang entstehenden Oxide. Eine im Deckelbereich des Metall­ zylinders 24 angebrachte Ableitung 32 dient zur Ableitung des Trägergases sowie des Reaktionsgases.In the upper section of the metal cylinder 24 , a filter 30 according to the invention is attached, which can be removed and replaced by means of the changing device 36 . The filter 30 serves to collect the oxides formed during the combustion process. A in the cover area of the metal cylinder 24 attached derivative 32 is used to discharge the carrier gas and the reaction gas.

Fig. 2 zeigt ein Flußdiagramm der einzelnen Verfahrensschritte des erfindungsgemäßen Verfahrens zur Bestimmung von Elementen mittels des Atomabsorptionsverfahren.A flow chart of the individual steps of Fig. 2 shows the method for determination of elements by means of the atomic absorption method.

Erfindungsgemäß werden einige Gramm der zu untersuchenden Probe in einen Keramiktiegel 16 eingebracht. Man gibt 0,8-1,2 g Wolframpulver zu. Der Tiegel 16 wird auf den Sockel 18 gestellt und in das Innere der Quarz­ röhre 12 gebracht. Die Zuleitungen für das Trägergas und das Reaktionsgas werden zugeschaltet. Als nächster Schritt wird nach Einschalten des Induktionsofens die Probe bei 2100 Grad Kelvin geschmolzen. Die Elemente werden als Ergebnisse der Verbrennung in einem Reaktionsgasstrom (02) in Form flüchtiger Gasoxide mittels des Trägergases transportiert und sind folglicherweise kondensiert. In Form von festen Partikeln werden Sie vom aschefreien Papierfilter 30, einem keramischen oder anderen Filter auf­ gefangen. Nach Beendigung des Verbrennungsvorgangs wird der Filter 30 aus dem Metallzylinder 24 herausgenommen und steht zur Analyse ganz oder teilweise zur Verfügung.According to the invention, a few grams of the sample to be examined are introduced into a ceramic crucible 16 . 0.8-1.2 g of tungsten powder are added. The crucible 16 is placed on the base 18 and brought into the interior of the quartz tube 12 . The feed lines for the carrier gas and the reaction gas are switched on. As the next step, the sample is melted at 2100 degrees Kelvin after switching on the induction furnace. The elements are transported as the results of the combustion in a reaction gas stream ( 02 ) in the form of volatile gas oxides by means of the carrier gas and are consequently condensed. In the form of solid particles, you are caught by the ashless paper filter 30 , a ceramic or other filter. After the combustion process has ended, the filter 30 is removed from the metal cylinder 24 and is available in whole or in part for analysis.

Anschließend wird ein Aliquot des Filters oder der ganze Filter in den Graphittiegel eines Atomabsorptionsspektrophotometers eingebracht und bekannterweise analysiert bzw. auf dem RF-Spektrometer analysiert.Then an aliquot of the filter or the entire filter is placed in the  Graphite crucible of an atomic absorption spectrophotometer introduced and known to be analyzed or analyzed on the RF spectrometer.

Optimale analytische Bedingungen und Ergebnisse werden beispielhaft für die Elemente As, Sn, Sb und Pb in den Tabellen 1 und 2 beschrieben.Optimal analytical conditions and results are exemplary for the elements As, Sn, Sb and Pb described in Tables 1 and 2.

Tabelle 1 zeigt das bestmögliche Verhältnis l/d (Fig. 1), d.h. das Verhältnis zwischen dem Filterabstand zur Verbrennungszone (l) und dem Quarzröhrendurchmesser (d), welcher den Verbrennungsraum begrenzt. Die in Tabelle 1 angeführten Ergebnisse wurden experimentell erarbeitet.Table 1 shows the best possible ratio l / d ( Fig. 1), ie the ratio between the filter distance to the combustion zone (l) and the quartz tube diameter (d), which limits the combustion chamber. The results listed in Table 1 were developed experimentally.

Tabelle 1 Table 1

Experimentell ermittelte l/d-Verhältnisse Experimentally determined l / d ratios

Während des Veraschungsprozesses im Graphitofen eines Atomabsorptions­ spektrophotometers wird die Filtermatrix des aliquoten Filterteiles verbrannt und vom Ofen weggeführt. Dadurch kann die unselektive Licht­ absorption in der Atomisierungsphase deutlich verringert oder sogar ganz ausgeschaltet werden.During the ashing process in the graphite furnace of an atomic absorption spectrophotometer is the filter matrix of the aliquot filter part burned and taken away from the oven. This allows the unselective light absorption in the atomization phase significantly reduced or even completely turned off.

Bei niedrigeren Veraschungstemperaturen erhöht sich die unselektive Licht­ absorption während der Atomisierungsphase. Bei zu hohen Temperaturen wird aufgrund von Evaporisation ein Elementverlust beobachtet.At lower ashing temperatures, the unselective light increases absorption during the atomization phase. At too high temperatures loss of element observed due to evaporation.

Die experimentell erbrachten Daten betreffend die optimale Veraschungs­ temperatur in einem Graphitofen eines Atomabsorptionsspektrophotometers können der Tabelle 2 entnommen werden.The experimental data regarding the optimal ashing  temperature in a graphite furnace of an atomic absorption spectrophotometer can be found in Table 2.

Tabelle 2 Table 2

Experimentell ermittelte Veraschungstemperaturen Ashing temperatures determined experimentally

In Tabelle 3 werden die analytischen Ergebnisse des erfindungsgemäßen Verfahrens mit denen des nach dem Stand der Technik am nächsten stehenden Verfahrens verglichen. Table 3 shows the analytical results of the invention Process with those closest to the prior art Procedure compared.  

Tabelle 3 Table 3

Vergleich des erfindungsgemäßen Verfahrens mit dem Verfahren des nächsten Standes der Technik Comparison of the method according to the invention with the method of the closest prior art

Claims (8)

1. Verfahren zur Bestimmung von Elementen mittels dem Atomabsorptions­ verfahren oder dem Röntgenfluoreszenzverfahren mit folgenden Schritten:
  • - Einbringen der Probe in einen Keramiktiegel unter Zugabe von Wolframpulver;
  • - Schmelzen der Probe in einem Induktionsofen bei 2 100°K; Auffangen der Elementoxide in einem Papierfilter oder Keramikfilter;
  • - Aufteilen des Papierfilters in aliquote Teile;
  • - Veraschung des Filters in einem Graphitofen eines Atomabsorptionsspektrophotometers;
  • - Analyse des keramischen Filters mit Röntgenfluoreszenzgerät; und
  • - Elementanalyse.
1. Method for determining elements using the atomic absorption method or the X-ray fluorescence method with the following steps:
  • - placing the sample in a ceramic crucible with the addition of tungsten powder;
  • Melting the sample in an induction furnace at 2 100 ° K; Collecting the element oxides in a paper filter or ceramic filter;
  • - dividing the paper filter into aliquots;
  • - Ashing the filter in a graphite furnace of an atomic absorption spectrophotometer;
  • - Analysis of the ceramic filter with an X-ray fluorescence device; and
  • - elemental analysis.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß zur Oxidation der Elemente Sauerstoff in den Induktionsofen eingeleitet wird.2. The method according to claim 1, characterized, that to oxidize the elements oxygen in the induction furnace is initiated. 3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß für den Transport der oxidierten Elemente zum Papierfilter oder keramischen Filter ein Trägergas in den Induktionsofen eingeleitet und verwandt wird.3. The method according to claim 1, characterized, that for the transport of the oxidized elements to the paper filter or  ceramic filter a carrier gas is introduced into the induction furnace and is used. 4. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Veraschungstemperatur im Graphitofen des Atomabsorptionsspektrophotometers bevorzugterweise 1100-1300°K beträgt.4. The method according to claim 1, characterized, that the ashing temperature in the graphite furnace of Atomic absorption spectrophotometers preferably 1100-1300 ° K is. 5. Vorrichtung zur Bestimmung von Elementen mittels des Atomabsorptions­ verfahrens oder des Röntgenfluoreszenzverfahrens unter Verwendung eines Induktionsofens und eines Atomabsorptionsspektrophotometers, dadurch gekennzeichnet, daß der Induktionsofen (10) eine Röhre (22), welche als Zuleitung für ein Trägergas dient sowie eine Röhre (26), welche als Zuleitung für das Reaktionsgas O2 dient, aufweist und im oberen Teil des Induktions­ ofens (10) ein Metallzylinder (24) angeordnet ist, welcher eine Wechselvorrichtung (28) für den Papierfilter bzw. Keramikfilter (30) sowie eine Ableitung (32) für die Gase im Innenraum des Induktionsofens enthält.5. Device for determining elements by means of the atomic absorption method or the X-ray fluorescence method using an induction furnace and an atomic absorption spectrophotometer, characterized in that the induction furnace ( 10 ) has a tube ( 22 ) which serves as a feed line for a carrier gas and a tube ( 26 ) , which serves as a feed line for the reaction gas O 2 , and in the upper part of the induction furnace ( 10 ) a metal cylinder ( 24 ) is arranged, which has a changing device ( 28 ) for the paper filter or ceramic filter ( 30 ) and a discharge line ( 32 ) for the gases inside the induction furnace. 6. Vorrichtung nach Anspruch 5, dadurch gekennzeichnet, daß der Filter (30) aus aschefreiem Papier besteht.6. The device according to claim 5, characterized in that the filter ( 30 ) consists of ash-free paper. 7. Vorrichtung nach Anspruch 5, dadurch gekennzeichnet, daß der Filter (30) aus Keramik besteht.7. The device according to claim 5, characterized in that the filter ( 30 ) consists of ceramic. 8. Vorrichtung nach Anspruch 5, dadurch gekennzeichnet, daß das Verhältnis zwischen dem Filterabstand zur Verbrennungszone (l) und dem Quarzröhrendurchmesser (d) bevorzugterweise zwischen 3,5 und 5 liegt.8. The device according to claim 5, characterized, that the ratio between the filter distance to the combustion zone (l) and the quartz tube diameter (d) preferably between 3.5 and 5 lies.
DE19893923983 1989-07-20 1989-07-20 Device for preparing a sample for a device for determining elements by means of atomic absorption methods or X-ray fluorescence methods Expired - Fee Related DE3923983C2 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
DE19893923983 DE3923983C2 (en) 1989-07-20 1989-07-20 Device for preparing a sample for a device for determining elements by means of atomic absorption methods or X-ray fluorescence methods
EP19900911638 EP0436008A1 (en) 1989-07-20 1990-07-12 Process and device for element determinations
JP51083190A JPH04503412A (en) 1989-07-20 1990-07-12 Element measurement method and device
PCT/EP1990/001146 WO1991001487A1 (en) 1989-07-20 1990-07-12 Process and device for element determinations

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19893923983 DE3923983C2 (en) 1989-07-20 1989-07-20 Device for preparing a sample for a device for determining elements by means of atomic absorption methods or X-ray fluorescence methods

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DE3923983A1 true DE3923983A1 (en) 1991-01-31
DE3923983C2 DE3923983C2 (en) 1999-02-25

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EP (1) EP0436008A1 (en)
JP (1) JPH04503412A (en)
DE (1) DE3923983C2 (en)
WO (1) WO1991001487A1 (en)

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EA014588B1 (en) * 2008-06-19 2010-12-30 Борис Арсентьевич Ревазов Method for determining metals in mineral raw material
CN106041037A (en) * 2016-05-31 2016-10-26 安泰科技股份有限公司 Preparation method for test sample for alloy powder performance analysis and special compound crucible
CN107213932A (en) * 2017-04-20 2017-09-29 东莞中子科学中心 A kind of Multi-example thermostat tested for small-angle scattering

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US8969832B2 (en) * 2010-07-15 2015-03-03 Beijing Titan Instruments Co., Ltd. Electrothermal vaporization atomic fluorescence spectroscopy and spectrometer for determination of cadmium
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RU199394U1 (en) * 2020-05-26 2020-08-31 Федеральный исследовательский центр "Пущинский научный центр биологических исследований Российской академии наук" (ФИЦ ПНЦБИ РАН) ELECTROTHERMAL TWO-STAGE ATOMIZER FOR ANALYTICAL SPECTROMETRY

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EA014588B1 (en) * 2008-06-19 2010-12-30 Борис Арсентьевич Ревазов Method for determining metals in mineral raw material
CN106041037A (en) * 2016-05-31 2016-10-26 安泰科技股份有限公司 Preparation method for test sample for alloy powder performance analysis and special compound crucible
CN107213932A (en) * 2017-04-20 2017-09-29 东莞中子科学中心 A kind of Multi-example thermostat tested for small-angle scattering

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